Biodiesel Production From Waste Cooking Oil Using Sulfuric Acid and Microwave Irradiation Processes

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Journal of Environmental Protection, 2012, 3, 107-113http://dx.doi.org/10.4236/jep.2012.31013 Published Online January 2012 (http://www.SciRP.org/journal/jep)

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Biodiesel Production from Waste Cooking Oil Using

Sulfuric Acid and Microwave Irradiation Processes

Prafulla D. Patil, Veera Gnaneswar Gude, Harvind K. Reddy, Tapaswy Muppaneni, Shuguang Deng*

Chemical Engineering Department, New Mexico State University, Las Cruces, USA.

Email: *[email protected]

Received July 30th, 2011; revised October 1st, 2011; accepted November 15th, 2011

ABSTRACT

A comparative study of biodiesel production from waste cooking oil using sulfuric acid (Two-step) and microwave-assisted transesterification (One-step) was carried out. A two-step transesterification process was used to produce bio-diesel (alkyl ester) from high free fatty acid (FFA) waste cooking oil. Microwave-assisted catalytic transesterificationusing BaO and KOH was evaluated for the efficacy of microwave irradiation in biodiesel production from waste cook-

ing oil. On the basis of energy consumptions for waste cooking oil (WCO) transesterification by both conventionalheating and microwave-heating methods evaluated in this study, it was estimated that the microwave-heating methodconsumes less than 10% of the energy to achieve the same yield as the conventional heating method for given experi-mental conditions. The thermal stability of waste cooking oil and biodiesel was assessed by thermogravimetric analysis(TGA). The analysis of different oil properties, fuel properties and process parametric evaluative studies of waste cook-

ing oil are presented in detail. The fuel properties of biodiesel produced were compared with American Society forTesting and Materials (ASTM) standards for biodiesel and regular diesel.

Keywords:Biodiesel; Waste Cooking Oil; Free Fatty Acid; Sulfuric Acid; Microwave-Assisted Transesterification

1. Introduction

The current methods to produce, convert and consume

energy derived from fossil fuels throughout the world are

not sustainable. Due to limited amounts of fossil fuels

and increasing concerns of global warming, there is ever-

growing urge to develop fuel substitutes that are renew-

able and sustainable. Biomass derived fuels such as me-

thane, ethanol, and biodiesel are well-accepted alterna-

tives to diesel fuels as they are economically feasible,

renewable, environmental-friendly and can be produced

easily in rural areas where there is an acute need for mo-

dern forms of energy.

Edible vegetable oils such as canola, soybean, and corn

have been used for biodiesel production and are proven

diesel substitutes [1,2]. However, a major obstacle in the

commercialization of biodiesel production from edible

vegetable oils is their high production cost, which is due

to the demand for human consumption. Reducing the

cost of the feedstock is necessary for biodiesels long-

term commercial viability. One way to reduce the cost of

this fuel is to use less expensive feedstocks including

waste cooking oils and vegetable oils that are non-edible

and/or require low harvesting costs. Waste cooking oil

(WCO), which is much less expensive than edible vege-

table oil, is a promising alternative to edible vegetable oil[3]. Waste cooking oil and fats set forth significant dis-

posal problems in many parts of the world. This envi-

ronmentally-threatening problem could be turned into

both economical and environmental benefit by proper

utilization and management of waste cooking oil as a fuel

substitute. Many developed countries have set policies

that penalize the disposal of waste cooking oil into waste

drainage [4]. The Energy Information Administration

(EIA) in the United States (USA) estimated that around

100 million gallons of waste cooking oil is produced per

day in USA, where about 9 pounds of waste cooking oil

are generated per person per year [5]. The estimatedamount of waste cooking oil collected in Europe is about

0.49 - 0.7 million gallons/day [6]. Waste cooking oil, as

an alternative feedstock for biodiesel, was studied with

different aspects such as optimization using supercritical

methanol (SCM) transesterification, process design and

technological assessment, fuel property analysis and cost

estimation approaches [7-9].

Biodiesel is derived from fats and oils either by

chemical or bio-chemical means [10]. There are at least

four ways in which oils and fats can be converted into

biodiesel, namely, transesterification, blending, micro-*Corresponding author.

Copyright 2012 SciRes.

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Biodiesel Production from Waste Cooking Oil Using Sulfuric Acid and Microwave Irradiation Processes108

emulsions and pyrolysis. Among these, transesterifica-

tion is the most commonly used method as it reduces the

viscosity of oil [11]. Biodiesel production by transesteri-

fication reaction can be catalyzed with alkali, acidic or

enzymatic catalysts. Alkali and acid transesterification

processes require less reaction time with reduced proc-essing costs as compared to the enzyme catalyst process

[12,13]. Alkali process yields high quantity and high

purity biodiesel in shorter reaction time [14]; however,

this process is not suitable for feedstock with high free

fatty acid (FFA) content. Therefore, a two-step trans-

esterification process (acid esterification followed by

alkali transesterification) was developed to remove high

free fatty acid (FFA) content and to improve the bio-

diesel yield. The long reaction time and low recovery of

catalyst were disadvantages of the two-step process. An

alternative method, namely the microwave-assisted cata-

lytic transesterification, has been developed that gives highbiodiesel yield and purity. Microwave-assisted trans-

esterification is an energy-efficient and a quick process

to produce biodiesel from different feedstocks [15,16].

Microwave-heating has been successfully applied to

synthesize porous materials and supported catalyst in our

previous research [17,18]. Microwave-assisted trans-

esterification of different feedstocks such as rapeseed oil,

cotton seed oil and waste cooking oils has been reported

by several researchers [15,19,20].

In this research, we have conducted several experi-

ments to compare the biodiesel production from waste

cooking oil using sulfuric acid (Two-step) and micro-

wave-assisted transesterification (One-step) processes.

Since waste cooking oil contains high FFA content, a

two-step process, acid esterification followed by alkali

transesterification was employed using methanol, sulfu-

ric acid and KOH catalyst. Microwave-assisted catalytic

transesterification using BaO and KOH was studied for

waste cooking oil to compare with the conventional

heating method. Energy requirements for both conven-

tional and microwave heating methods and product se-

paration times were compared.

2. Methodology

Waste cooking oil (WCO) was collected from a local

restaurant in Las Cruces, NM. Potassium hydroxide

flakes, methanol (AR Grade), and diethyl ether were

procured from Fisher Scientific, New Jersey. Sulfuric

acid (98% pure) was procured from Acros Organics,

New Jersey. The mixture was stirred at the same speed

for all test runs. All experiments of transesterification

reaction were performed in a 250 mL round-bottom flask

equipped with a water-cooled reflux condenser. A hot

plate with magnetic stirrer arrangement was used for

heating the mixture in the flask. The microwave-assisted

transesterification was performed using a modified do-

mestic microwave oven (with an output power of 800 W).

The microwave oven was modified and fitted with a

temperature reader, an external agitator and a water-

cooled reflux condenser.

2.1. Characteristics of Waste Cooking Oil

The quality of oil is expressed in terms of the physico-

chemical properties such as acid value, saponification

value, and iodine value. The saponification value of

waste cooking oil (WCO) was reported as 186.3 (mg

KOH/g). The acid value of waste cooking oil was found

to be 17.41 mg KOH/gm. It has been reported that trans-

esterification would not occur if FFA content in the oil

were above 3 wt% [21].

2.2. Transesterification Reaction

The transesterification process was widely used in bio-diesel production from different biomass materials. The

process consists of two steps namely, acid esterification

and alkali transesterification [22]: Step 1: Acid esterifi-

cation: Acid esterification reduces the FFA value of un-

refined oil using an acid catalyst. Step 2: Alkali trans-

esterification: After removing the impurities of the pro-

duct from the Step 1, it is transesterified to monoesters of

fatty acids using an alkali catalyst.

The mechanism of synthesis of biodiesel via two-step

transesterification process is represented as

Acid Esterification (Step 1)

RCOOH + CH3OH RCOOH3 + H2OH

2SO

4

Acid Transesterification (Step 2)

CH2OOCR1

R2COOH3CHOOCR2

CH2OOCR3

Triglyceride Methanol Methyl Ester Glycerol

+ 3CH3OHKOH

R1COOH3

R3COOH3

+ CHOH

CH2OH

CH2OH

For microwave transesterification procedure, the cal-

culated amount of waste cooking oil was added to thepremixed solution of methanol and catalysts (KOH and

BaO). The mixture was then subjected to the microwave

irradiation with exiting power of 800 W, under a matrix

of conditions: methanol to oil molar ratio of 6:1 to 15:1;

catalyst concentrations in the range 1 - 2 wt% of oil with

constant reaction time of 6 min. The purification and

separation steps (downstream procedure) are described

elsewhere [23].

2.3. Analysis of Biodiesel

For the quantification of reaction products, the samples


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Biodiesel Production from Waste Cooking Oil Using Sulfuric Acid and Microwave Irradiation Processes 109

were analyzed by a gas chromatography-mass spec-

trometry (GC-MS) system incorporated with an Agilent

5975 C mass-selective detector (MSD) and an Agilent

7890 A gas chromatograph equipped with a capillary

column (HP-5 MS, 5% phenyl methyl silox 30 m 250

m 0.25 m nominal). Methyl heptadecanoate (10.00mg; internal standard) was dissolved in 1 mL heptane to

prepare the standard solution. Approximately 55 mg

methyl ester was dissolved in 1 mL standard solution for

GC analysis. Approximately 1 L sample was injected

into the GC. Helium was used as the carrier gas. The

injection was performed in splitless mode. The parame-

ters of the oven temperature program consist of: start at

80C with 10C/min intervals up to 180C (1 min) and up

to 255C with 15C/min intervals (2 min). The Fatty acid

methyl ester (FAME) content was calculated by use of

the equation:

100%

EI EI EI

EI

A A C VC

A W

The biodiesel yield is apparently same to that of the

FAME Content (%) calculated quantitatively by GC-MS

[24].Where A total peak area of methyl ester,AEI

peak area of methyl heptadeconoate, CEIconcentration

(mg/mL) of standard solution (methyl heptadecanoate),

VEIvolume (mL) of standard solution (methyl hepta-

decanoate) and Wweight (mg) of sample. From GC-

MS and TIC analysis, it can be noted that waste cooking

biodiesel contains major proportion of unsaturated fatty

acids.

3. Results and Discussion

3.1. Sulfuric Acid Process(Two-Step Transesterification)

Acid esterification reaction was studied for four different

molar ratios. The sulfuric acid catalyst amount was var-

ied in the range of 0.3% to 2%. These percentages are

based on volume of the oil used for the acid esterification

reaction. The catalyst amount also affects the yield of

process is shown in Figure 1. The acid-catalyst process

attained maximum yield for waste cooking oil at 0.5%catalyst concentration. It was observed that the yield

started to decline when the catalyst concentration was

increased to above 0.5%.

Methanol to oil molar ratio was varied for waste

cooking oil within the range of 3:1 to 9:1. The maximum

biodiesel yield for waste cooking oil was found at the

methanol to oil molar ratio of 6:1 in acid esterification. In

alkali transesterification, the maximum yield for waste

cooking oil was obtained at the methanol to oil molar

ratio of 9:1. The yield remains the moreover same with

further increase in the methanol to oil molar ratio. The

excess methanol in the ester layer can be removed by

distillation. Canakci and Van Gerpan [25] advocate the

use of large excess quantities of methanol (15:1-35:1)

while using the sulphuric acid as catalyst. Figure 2

shows the methanol to oil molar ratio effect in alkali

transesterification (Step 2). At higher levels, an excess

methanol amount may reduce the concentration of the

catalyst in the reactant mixture and retard the transesteri-

fication reaction [26].

An alkali catalyst was studied in the range of 0.3% to

2.5% using KOH as an alkali catalyst. The influence of

the alkali catalyst amount on the yield is shown in Fig-

ure 3. The maximum yield was achieved for waste

cooking oil at 2% of catalyst loading. During the experi-

ments, it was also observed that transesterification could

not take place properly with an insufficient amount of an

alkali catalyst loading. The production yield slightly de-

creased above 2% of catalyst loading. At higher concen-trations, the intensification of mass transfer became more

important than increasing the amount of catalyst. The

reaction temperature effect on the yield was studied in

the temperature range of 40C to 100C at atmospheric

40

50

60

70

80

90

100

0 0.5 1 1.5 2 2

Acid Conc.( v/v %)

BiodieselYield(%)

.5

Figure 1. Effect of acid concentration on biodiesel yield

(Step 1) in sulfuric acid process.

0

20

40

60

80

100

0 2 4 6 8 10 12

MeOH:Oil (Step 2)

BiodieselYield(%

)

14

Figure 2. Effect of molar ratio on biodiesel yield (Step 2) in

sulfuric acid process.


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0

20

40

60

80

100

0 0.5 1 1.5 2 2.5 3

Alkali Conc. (wt%)

Biodiesel

Yield(%)

Figure 3. Effect of alkali catalyst amount on biodiesel yield

(Step 2) in sulfuric acid process.

pressure. The maximum yield was obtained at a tem-

perature of 80C for waste cooking oil.

3.2. Microwave Catalytic Transesterification

The effect of methanol to oil molar ratio and catalyst

concentration (BaO and KOH) on waste biodiesel yield

using microwave method. Methanol-to-oil ratios of 6:1,

9:1, 12:1, and 15:1 were tested for both catalysts. In this

study, for homogeneous catalysts (KOH), a molar ratio

of 9:1 and 2% catalyst were found to be effective with

maximum biodiesel yield of 92% (Figure 4). For BaO, a

maximum biodiesel yield of 96% was obtained for 12:1

methanol to oil molar ratio and 2% catalyst concentration

(Figure 5). It was observed for homogeneous catalyst

that when the amount of methanol-to-oil molar ratio wasincreased over 9:1, excess methanol started to interfere in

the separation of glycerin due to an increase in the solu-

bility and resulted in lower biodiesel yield [27].

In combine effect of excess alcohol and KOH catalyst

leads to saponification resulting in lower biodiesel yield

and lower biodiesel quality. An advantage associated

with heterogeneous catalysts is that they can be recov-

ered and reused several times. For homogeneous cata-

lysts, the biodiesel separation and catalyst recovery from

reaction mixture can be laborious. The reactivity of BaO

catalyst was found to be quite different than KOH cata-

lyst as it posses different catalytic activity, basicity, leach-

ing tendency, and specific surface area, which influence

the transesterification of oil [28].

Energy requirements for the two heating methods (mi-

crowave and conventional) for waste cooking oil trans-

esterification are presented in Table 1. It can be noted

that that 6 min were sufficient for microwave heating

while 105 min were required for conventional heating to

achieve comparable biodiesel yields. This large differ-

ence in reaction time can be attributed to the limitations

of conventional heating in which the energy is first util-

ized to increase the temperature of the reaction vessel

and the higher temperature of the reaction vessel results

in higher heat losses to the ambient. The energy required

by the conventional method is found to be around 11

times greater than that by the microwave method to

achieve same biodiesel yield for waste cooking oil. From

our previous study for camelina oil transesterification, it

was concluded that proper power dissipation control re-sulted in effective use of the microwave energy and fur-

ther reduction in energy requirements [23].

40

50

60

70

80

90

100

4 6 8 10 12 14 16

MeOH:Oil

Biodieselyield

(%

)

KOH 1%

KOH 1.5%

KOH 2%

Figure 4. Effect of methanol to oil molar ratio and catalyst

concentration (KOH) on biodiesel yield using microwave

method.

40

50

60

70

80

90

100

110

4 6 8 10 12 14 1

MeOH :Oil

BiodieselYield(%

)

6

BaO 1%

BaO 1.5%

BaO 2%

Figure 5. Effect of methanol to oil molar ratio and catalyst

concentration (BaO) on biodiesel yield using microwave

method.

Table 1. Comparison of energy consumptions for biodieselproduction from waste cooking oil by two methods.

Microwave

heating

Conventional

heatingCatalyst

Energy dissipated (J/s) 800 500

Time of reaction (s) 360 6300

% Power emitted 100 100

Total energy required (kJ) 288 3150

Ratio 1 10.93

Biodiesel yield (%) 92 92

KOH


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Biodiesel Production from Waste Cooking Oil Using Sulfuric Acid and Microwave Irradiation Processes


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111

The major benefits of microwave-assisted transesteri-

fication over conventional heating are: 1) Rate Enhance-

ment: reaction times can be drastically reduced from hours

to minutes; 2) Increased yield: shorter reaction time mini-

mizes unwanted side reactions; 3) Improved purity: less

by-products result in simplified purification.

recorded that 0.9% loss of sample at 125C, 41.54% loss

at 232C and 98% loss at 460C. The percentage of bio-

diesel and waste cooking oil in a sample could be calcu-

lated from the TGA plot of the sample taking into ac-

count the first derivative of the weight change of the

sample mixture.

In addition, the mass loss recorded for biodiesel at

125C correlates the mass percentage of biodiesel present

in the sample. Likewise, the mass loss associated with

waste cooking oil (ca. 325C) correlates to the mass per-

centage of waste cooking oil in the sample. Because of

these temperatures vary by a relatively large value (approx

200C), this method should be quite effective in distin-

guishing biodiesel from waste cooking oil.

3.3. Thermogravimetric Analysis of WasteCooking Oil and Biodiesel

Thermogravimetric analysis (TGA) is a technique for

characterizing thermal stability of a material (compound

or mixture) by measuring changes in its physicochemical

properties expressed as weight change as a function of

increasing temperature [29]. TGA is a simple, convenient,

and economical method for monitoring biodiesel produc-

tion.3.4. Fuel Properties of Methyl Esters

Figure 6 shows the TGA plot for waste cooking oil,

biodiesel and mixture of oil and biodiesel (50% - 50%).

TGA was performed on PerkinElmer Pyris 1 TGA in-

strument. The temperature range employed was 25C -

600C. The mass of the waste cooking biodiesel starts to

decrease at approximately after 125C - 130C, and this

step was attributed to vaporization of biodiesel, and the

second step started to decrease at 232C, and it may be

due to some waste cooking oil that was not transesteri-

fied. TGA curve of waste cooking biodiesel did not show

any step afterwards, confirmed that the transesterification

reaction was complete. Similarly, evaporation of waste

cooking oil starts at approximately 325C. TGA curve for

waste cooking oil and biodiesel (50% - 50%) mixtureconfirmed the combine effect of both samples at respec-

tive temperatures as discussed above. For mixture, it was

The fuel properties of biodiesel from waste cooking oil

(WCO) obtained from microwave process with testing

methods are given in Table 2. The viscosities of bio-

diesel from waste cooking oil was closer to that of vis-

cosity of regular diesel i.e. 2.6 mm2/s. Hence, no hard-

ware modifications are required for handling this fuel

(biodiesel) in the existing engine. The calorific value of

waste cooking oil ester was reported in the range of

45.08 - 45.24 MJ/kg. The cetane number was found to be

higher than ASTM standards for biodiesel. Higher cetane

number indicates good ignition quality of fuel. The pour

point of waste cooking biodiesel was found to be in be-

tween 4C - 1C. This pour point might give rise to low

running problems in cold season. This problem could beovercome by the addition of suitable pour point depres-

sants or by blending with diesel oil.

Figure 6. Overlay of thermogravimetric curves for waste cooking oil, biodiesel and mixture (50% - 50%) of waste cooking oil

and biodiesel.


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Table 2. Properties of methyl ester from waste cooking oil.

PropertiesWaste

Cooking Oil

Waste cooking

methyl ester

Biodiesel standard

ASTM D 6751-09Regular diesel Testing method

Specific Gravity 0.92 0.87 - 0.88 0.86 - 0.90 0.85 ASTM D4052

Viscosity (mm2/s) at 40C 28.8 2.25 - 3.10 1.9 - 6.0 2.6 ASTM D445

Calorific Value (MJ/kg) 44.44 45.08 - 45.24 Report 42 ASTM D240

Cetane Number 32.48 55.45 - 56.10 47 min. 46 ASTM D613

Pour Point (C) 12 4 to 1 Report 20 ASTM D97

4. Conclusion

The production of fuel quality biodiesel from low-cost

high FFA waste cooking oil was investigated. A two-step

transesterification process was used to convert the high

free fatty acid oil to its ester. Microwave-assisted trans-

esterification of waste cooking oil using heterogeneousand homogeneous was investigated for optimum reaction

conditions. The preliminary experimental study per-

formed in this work has demonstrated that the micro-

wave-heating method is energy-efficient and better than

the conventional heating method.

5. Acknowledgements

This project was partially supported by US Department

of Energy (DE-EE0003046) and US Air Force Research

Laboratory (FA8650-11-C-2127).

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Biodiesel Production From Waste Cooking Oil Using Sulfuric Acid and Microwave Irradiation Processes

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